ArticleLiterature Review

Advances in Sample Preparation Methods for Pesticide Residue Analysis in Medicinal Plants: A Focus on Nepal

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Abstract

Medicinalplantsafetyisarisingchallengeworldwideduetothecontinuedoveruse ofpesticidestotheirmaximumresiduelimits.Duetothehighdemandformedicinal plants, theirproduction isbeing increasedandsometimesprotectedbypesticide use.Theanalysisoftheseresiduesrequiresrobustanalyticalmethodstoensurethe safetyandqualityofmedicinalplants.Developingeffectivesamplepreparationfor detectingpesticidesischallenging,duetotheirdiversenatures,classes,andphysicochemical characteristics.Hence, existingtechniquesandstrategiesareneededto improve the reliabilityof the results. The reviewdiscusses thecurrent stateof samplepreparationtechniques, analyticalmethods, and instrumental technologies employed in pesticide residue analysis in medicinal plants. It highlights the challenges, limitations, andadvancements inthe field, providing insights intothe analytical strategies used to detect and quantify pesticide residues. Reliable, accessible, affordable, andhigh‐resolutionanalytical procedures areessential to ensure that pesticide levels inmedicinal plants are effectively regulated. By understanding thecomplexitiesof pesticide residueanalysis inmedicinal plants, this reviewarticleaims tosupport theconservationofmedicinal plant resources, promotepublichealth,andcontributetothedevelopmentofsustainablestrategies for ensuring thesafetyandqualityofmedicinal plants inNepal. The findingsof thisreviewwillbenefitresearchers,policymakers,andstakeholders involvedinthe conservationofmedicinalplantresourcesandthepromotionofpublichealth. KEYWORDS analytical techniques,medicinalplants,pesticides, samplepreparation, toxicity

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The measurement of 23 organochlorine, organophosphorus, and pyrethroid pesticides in typical traditional Chinese medicine (TCM), flos lonicerae, was made using gel permeation chromatography (GPC) purification and gas chroma-tography-mass spectrometry (GC-MS) detection. The pesticides were extracted with ultrasonic device and 5.0 mL mix-ture of ethyl acetate and cyclohexane (1:1, v/v). Coextractants from sample matrices which may have interfere to the qualitative and quantitative analysis, such as pigments, were removed using GPC purification. Simultaneous full scan and selective ion monitor (scan/SIM) mode for GC-MS was used for qualitative and quantitative analysis, which pro-vided retention time and characteristic fragments ratio for each pesticide so as to positively identify each analyte. Rela-tive standard deviations (RSDs) were within 7.7% (5.0 -22.5 µg/kg, n = 3). The recoveries of pesticide standards at the spiked concentration of 5.0 -22.5 µg/kg were between 87.1% and 110.9%. Limits of detection (LODs) for the analytes were 0.16 -3.2 µg/kg, which could meet the demand of routine analysis and TCM quality control.
Article
We conducted this study in order to assess the pesticide residues in vegetables and examine the related human health risk. Therefore, residues of 23 pesticides (organophosphates, organochlorines, acaricides, fungicides, and insecticides of biological origin) were analysed in the three main vegetable crops grown in Southern Nepal: 27 eggplant, 27 chilli and 32 tomato samples representing (i) conventional (N = 67) and ii) integrated pest management (IPM) fields (N = 19). Pesticide residues were found in 93% of the eggplant samples and in all of the chilli and tomato samples. Multiple residues were observed in 56% of the eggplant samples, 96% of chilli samples and all of the tomato samples. The range (µg/kg) of total detected pesticide residues in eggplants, chillies and tomatoes was 1.71–231, 4.97–507, 13.1–3465, respectively. The most frequently detected pesticides in these vegetables were carbendazim and chloropyrifos. Pesticide residues in 4% of the eggplant, 44% of the tomato and 19% of the chilli samples exceeded the EU maximum residue limits (MRLs). The residues of triazophos, omethoate, chloropyrifos and carbendazim exceeded the EU MRLs. Compared to chilli and eggplant crops, more carbendazim was sprayed onto tomato crops (p < 0.05). We assessed adolescent and adult dietary exposure using hazard quotient (HQ) and hazard index (HI) equations for the identified pesticides. HQ> 1 was observed for chloropyrifos, triazophos and carbendazim in eggplants; profenofos, triazophos, dimethoate, omethoate, chloropyrifos and carbendazim in tomatoes; and dichlorvos and chloropyrifos in chillies. Of all of the HQs, the highest acute HQ (aHQ) was for triazophos (tomato) in adolescents (aHQ=657) and adults (aHQ=677), showing the highest risks of dietary exposure. The cumulative dietary exposure showed a higher HI for organophosphates (HI>83) and a lower HI for organochlorines, acaricides and biological insecticides (HI<1). The concentration of pesticide residues in the vegetable crops from the IPM field was considerably lower, suggesting a greater ability of IPM systems to reduce the dietary risks from exposure to pesticides.
Article
The safety of Traditional Chinese Medicine (TCM) is of concern worldwide. Herein, Paeoniae Radix Alba, Chaenomelis Fructus and Moutan Cortex, representing three medicinal components, were subjected to toxicological analysis to investigate possible pesticide contamination. Exposure using a point estimate model identified 47 residues that were simultaneously validated by the QuEChERS-UPLC-MS/MS method, which is sufficiently reliable for measuring residue concentrations. Of the 313 samples tested, 94.57% contained pesticide residues, with concentrations ranging from 0.10 to 1199.84 μg kg⁻¹, of which >83.17% contained 4–15 different residues. Carbendazim was the most frequently detected pesticide (>85%), and procymidone, pendimethalin and phoxim were also abundant (median concentration = 15.33–623.12 μg kg⁻¹). Risk assessment based on the hazard quotient/hazard index (HQ/HI) approach revealed that exposure to pesticide residues in all three TCMs (95th percentile) were far below levels that might pose a health risk. However, insecticides contributed to cumulative exposure, especially phoxim, and worryingly, several banned pesticides were detected. The results are of theoretical and practical value for evaluating the safety TCMs, and could improve their quality and safety.
Article
Currently used pesticides (CUPs) represent one of the largest intentional inputs of potentially hazardous compounds into agricultural soils. Subsequently, pesticide residues (PRs) and their transformation products (TPs) persist in agricultural soils, occurring in diverse mixtures of compounds in various concentrations. In this study, measured environmental concentrations (MECs) of CUP residues and TPs, originated from previous growing seasons in agricultural soils of the Czech Republic, were used to characterize the environmental risk for agroecosystems. Toxicity exposure ratios (TERs) were calculated using predicted no-effect concentrations (PNECs) and MECs in order to identify single pesticide residues risk to in-soil invertebrates and microorganisms. Ecological risk assessment (ERA) for the mixtures of pesticide residues at each monitored site was assessed using a risk quotient (RQ) method and considering concentration addition among components in the mixtures. The compilation of ecotoxicity data to derived PNECs for in-soil organisms clearly showed data gaps mainly for triazine and chloroacetanilide TPs. In addition, chronic toxicity data for in-soil invertebrates at different trophic levels are not available for 30% of monitored CUPs. The ERA revealed that pesticide residues in soil pose a risk at 35% of the sites (RQ ≥ 1). Among measured pesticides, epoxiconazole, atrazine-2-hydroxy, carbendazim, dimoxystrobin, terbuthylazine and difenoconazole were the main contributors to the overall pesticide mixture toxicity. The measured levels of epoxiconazole together with the frequent presence in soils represent a risk for the agroecosystems. Further assessment of higher tiers of ERA should be considered and prioritized in the pesticides risk management.
Article
Spices are known as difficult matrices that contain variable amounts of fats, piperine or many other matrix constituents. The increasing sensitivity of new GC-MS/MS platforms opens new approaches to analyze pesticide residue in complex matrices such as spices, by sample dilution. The aim of this work is to develop and validate an effective multiresidue method for the analysis of pesticide residues in spices by GC-MS/MS. In this paper, we highlight the importance of reducing matrix interferences generated from co-extractive components of spices. Moreover, we emphasize the concern of obtaining clean extracts requiring less instrument maintenance. By evaluating the total ion chromatograms (TIC) on GC-Orbitrap-MS of different extracts using various sorbents, QuEChERS citrate using EMR-Lipid sorbent resulted in the cleanest extract among Z-Sep, Primary secondary amine (PSA), Oasis® Prime HLB, and Supelclean™ Ultra cartridges that consist of a top bed of PSA, C18 and Grashsphere™ 2031 and a bottom bed of Z-Sep. Later, the analyses were performed on a GC-QQQ-MS/MS, applying a 15 min runtime method covering 205 compounds. The samples were diluted 25 times before the injection bearing in mind that the instrumental LOQs reached (iLOQ) were 2 ng g-1 and the method LOQs (mLOQ) were 50 ng g-1. Good recoveries between 70 and 120% with RSDs lower than 20% were observed for 90% of the compounds in black pepper and for 83% of the compounds in cayenne pepper. To demonstrate the applicability of the proposed method, 50 real dried and non-dried spice samples were analyzed. The most detected pesticides were metalaxyl, chlorpyrifos, tebuconazole, ethion, and chinomethionate.
Article
A method was established for the simultaneous determination of 116 pesticide residues in Notoginseng Radix et Rhizome with a combination of the modified QuEChERS method and GC–MS/MS. The sample was extracted with acetonitrile, cleaned up by primary–secondary amine and octadecyl-modified silica (C18) sorbents and determined by GC–MS/MS in multireaction monitoring mode. Matrix-matched calibration coupled with internal standard method was applied to compensate for the matrix effect and to quantify the pesticides. The results of all the 116 pesticides showed good linearity in the respective linear range with correlation coefficients (r²) > 0.99. The method limits of quantification were between 0.01 and 0.05 mg kg⁻¹. The recoveries were between 64.3 and 119.4%, with RSD values typically lower than 18.3% at three spiked levels of 0.05, 0.10 and 0.20 mg kg⁻¹. The validated methodology is easy, fast, highly accurate, reliable and sensitive for monitoring and quantification of the 116 pesticide residues in Notoginseng Radix et Rhizoma. In 180 batches of real samples, 11 pesticides were detected and among these quintozene and cyfluthrin were in excess of the standard of European Union maximum residue level for herbs.
Article
A novel screening and quantitation method is reported for non-target multiresidue analysis of pesticides using ultra-HPLC-quadrupole-Orbitrap mass spectrometry in spice matrices, including black pepper, cardamom, chili, coriander, cumin, and turmeric. The method involved sequential full-scan (resolution = 70,000), and variable data independent acquisition (vDIA) with nine consecutive fragmentation events (resolution = 17,500). Samples were extracted by the QuEChERS method. The introduction of an SPE-based clean-up step through hydrophilic-lipophilic-balance (HLB) cartridges proved advantageous in minimizing the false negatives. For coriander, cumin, chili, and cardamom, the screening detection limit was largely at 2 ng/g, while it was 5 ng/g for black pepper, and turmeric. When the method was quantitatively validated for 199 pesticides, the limit of quantification (LOQ) was mostly at 10 ng/g (excluding black pepper, and turmeric with LOQ = 20 ng/g) with recoveries within 70-120%, and precision-RSDs <20%. Furthermore, the method allowed the identification of suspected non-target analytes through retrospective search of the accurate mass of the compound-specific precursor and product ions. Compared to LC-MS/MS, the quantitative performance of this Orbitrap-MS method had agreements in residue values between 78-100%.
Article
Higher matrix interference makes the multi-residue pesticide analysis in spices more challenging. A simple, sensitive, and robust large-scale multi-residue method was developed for the rapid analysis of 243 pesticides in cardamom matrix by gas chromatography tandem mass spectrometry (GC-MS/MS). Prehydration of cardamom in 1:4 sample:water for 30 min improved the homogeneity and extractability. QuEChERS extraction followed by cleanup with 25 mg primary secondary amine, 100 mg C18, and 10 mg graphitized carbon black to 1 ml supernatant was used for sample preparation. Reconstitution of final extract in ethyl acetate reduced matrix co-extract up to 60%. The method was validated according to the SANTE/11,945/2015 guidelines. The limit of quantification was ≤0.01 mg kg(-1), and the recovery was within 70.0-120.0%, with ≤20% RSD for the majority of pesticides. The method was used for screening market samples, and the detected residues were devoid of any risk of acute toxicity related to dietary exposure.
Article
A simple and efficient multi residue method was developed, for the analysis of 160 pesticides by GC-MS/MS in herbal plants. The developed method employs pesticide residue extraction by EtAC/ n. hexane (6:4) with a cleanup step using florisil/ PSA mixture. The optimized conditions have resulted in lower co-extracted matrix components than those extracted using EtAC or MeCN (QuEChERS method), according to FTIR and full scan GC/MS analyses. In addition, the developed method (EtAC/ Hexane) eliminates the evaporation step that is usually performed when using MeCN as an extraction solvent prior to the GC-MS/MS injection. The developed method was fully validated on chamomile, based on SANTE/11945/2015 guidelines. Where, intraday recoveries were estimated at three concentration levels of 10, 50 and 250 μg kg⁻¹. However, interday recoveries have also been carried out, at 250 μg kg⁻¹. In addition, intraday recoveries were estimated for two other herbal plants (thyme and marjoram), at 250 μg kg⁻¹. Three point calibration mixtures were prepared in ethyl acetate solvent and in the blank extracts of chamomile, thyme, and marjoram, in order to check the linearity and matrix effect. The average recoveries for most of the studied pesticides ranged from 70 to 100% at 50 and 250 μg kg⁻¹ with relative standard deviations below 20%. The validated method was successfully applied for determination of pesticide residues in 20 herb samples, collected from the Egyptian market.
Article
Gas and liquid chromatography coupled to triple quadrupole tandem mass spectrometry are currently the most powerful tools employed for the routine analysis of pesticide residues in food control laboratories. However, whatever the multiresidue extraction method, there will be a residual matrix effect making it difficult to identify/quantify some specific compounds in certain cases. Two main effects stand out: (i) co-elution with isobaric matrix interferents, which can be a major drawback for unequivocal identification, and therefore false negative detections, and (ii) signal suppression/enhancement, commonly called the “matrix effect”, which may cause serious problems including inaccurate quantitation, low analyte detectability and increased method uncertainty. The aim of this analytical study is to provide a framework for evaluating the maximum expected errors associated with the matrix effects. The worst-case study contrived to give an estimation of the extreme errors caused by matrix effects when extraction/determination protocols are applied in routine multiresidue analysis. Twenty-five different blank matrices extracted with the four most common extraction methods used in routine analysis (citrate QuEChERS with/without PSA clean-up, ethyl acetate and the Dutch mini-Luke “NL” methods) were evaluated by both GC-QqQ-MS/MS and LC-QqQ-MS/MS. The results showed that the presence of matrix compounds with isobaric transitions to target pesticides was higher in GC than under LC in the experimental conditions tested.
Article
A new reliable, fast and highly sensitive method based on ultra-high performance liquid chromatography tandem mass spectrometry has been developed and validated for the determination of 28 carbamates in aromatic herbs. A modified QuEChERS-based method was optimized for the extraction of carbamate residues from a wide variety of fresh herbal products. The proposed method allowed recoveries higher than 72%, achieving quantification limits of 2 μg kg⁻¹, therefore below maximum residue limits established for this type of samples. The combination of QuEChERS with UHPLC-MS/MS introduces a high-throughput methodology for the monitoring of these residues in this type of matrices scarcely explored. The analysis of the real samples revealed that several samples sold in the European Union and in the North West region of Cameroon contain pesticides in concentrations below the maximum residue limits.
Article
The aim of this research was to adapt the QuEChERS method for routine pesticide multiresidue analysis in edible vegetable oil samples using gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). Several clean-up approaches were tested: (a) D-SPE with Enhanced Matrix Removal-Lipid (EMR-Lipid™); (b) D-SPE with PSA; (c) D-SPE with Z-Sep; (d) SPE with Z-Sep. Clean-up methods were evaluated in terms of fat removal from the extracts, recoveries and extraction precision for 213 pesticides in different matrices (soybean, sunflower and extra-virgin olive oil). The QuEChERS protocol with EMR-Lipid d-SPE provided the best reduction of co-extracted matrix compounds with the highest number of pesticides exhibiting mean recoveries in the 70-120% range, and the lowest relative standard deviations values (4% on average). A simple and rapid (only 5min) freeze-out step with dry ice (CO2 at -76°C) prior to d-SPE clean-up ensured much better removal of co-extracted matrix compounds in compliance of the necessity in routine analysis. Procedural Standard Calibration was established in order to compensate for recovery losses of certain pesticides and possible matrix effects. Limits of quantification were 10μgkg(-1) for the majority of the pesticides. The modified methodology was applied for the analysis of different 17 oil samples. Fourteen pesticides were detected with values lower than MRLs and their concentration ranged between 10.2 and 156.0μgkg(-1).
Article
Ethnopharmacological relevance: The rich floral and ethnic composition of eastern Nepal and the widespread utilization of locally available medicinal plants offer remarkable opportunity for ethnomedicinal research. The present paper aims to explore medicinal plant diversity and use in the remote villages of eastern Nepal. It also aims to evaluate ethnopharmacological significance of the documented use reports and identify species of high indigenous priority. Materials and methods: The study was undertaken in four villages located in the Sankhuwasabha district in eastern Nepal. Ethnomedicinal information was collected through structured interviews. The homogeneity of informant's knowledge and the relative importance of documented medicinal plants were validated by informant consensus factor and use value, respectively. Species preference for treatment of particular diseases was evaluated through fidelity level. Results: We reported medicinal properties of 48 species belonging to 33 families and 40 genera, for the treatment of 37 human ailments. The uses of 10 medicinal plants were previously undocumented. The informant consensus factor (FIC) ranged between 0.38 and 1 with about 50% of values greater than 0.80 and over 75% of values greater than 0.70, indicating moderate to high consensus among the informants on the use of medicinal plants in the region. Swertia chirayita was the most preferred species with significantly high use values, followed by Paris polyphylla and Neopicrorhiza scrophulariiflora. Conclusions: The remote villages in eastern Nepal possess rich floral and cultural diversity with strong consensus among informants on utilization of plants for local healthcare. The direct pharmacological evidence for medicinal properties of most species indicates high reliability of documented information. Careful and systematic screening of compounds isolated from these plants could possibly provide good opportunity for the discovery of novel medicines to treat life-threatening human diseases. We recommend prioritization of medicinal plants and reinforcement of existing cultivation practices for sustainable management of high-priority species.
Article
In this article we have evaluated the performance of different sorbents for the cleanup step in multiresidue pesticide analysis in fatty vegetable matrices using QuEChERS methodology. The three different matrices tested (olive oil, olives and avocado) were partitioned using acetonitrile prior to cleanup step. Afterwards, the supernatant was purified using different sorbents: C18+PSA (primary secondary amine), Z-Sep+ (zirconium oxide and C18 dual bonded to silica), Z-Sep (zirconium oxide bonded to silica) and a novel sorbent Enhanced Matrix Removal-Lipid (EMR) whose composition has not been disclosed. The different cleanup strategies were compared for a group of 67 representative pesticides in terms of recovery rates, matrix effects, extract cleanliness and precision using ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The best extraction efficiencies in olive oil matrix were obtained using EMR, while the results for olives and avocado were pretty similar amongst the different sorbents with an overall lower performance in terms of matrix effects and recovery rates compared to olive oil data, particularly in olives due to the higher complexity and concentration of coextracted species. On the other hand, the average reproducibility was clearly better when EMR sorbent was employed in all selected matrices for most pesticides (RSD < 10% for 45, 52, and 56 pesticides in avocado, olives and olive oil respectively). The best results in terms of matrix effects were also obtained with EMR; with signal suppression lower than 20% for 79%, 16% and 51% of pesticides tested in olive oil, olives and avocado respectively. Using EMR as cleanup sorbent, limits of quantitation using UHPLC-MS/MS, ranged from 0.10 to 90 μg kg−1, allowing their determination at the low concentration levels demanded by current olive oil regulations in most cases.
Article
The present study is focused on the development of an analytical method for the simultaneous analysis of seventy-four pesticides belonging to different chemical classes (organochlorines, organophosphates, pyrethroids, dinitroanilines, dicarboximides, triazoles, etc.) in Chinese material medica. The samples were extracted according to the acetate QuEChERS protocol. To reduce the amount of co-extracted compounds, n-hexane instead of acetonitrile was employed as the extraction solvent. To improve the overall recoveries of problematic basic and base-sensitive compounds, sodium acetate was used to adjust the pH to a neutral condition, and florisil combined with octadecyl-modified silica (C18) were utilized in the cleanup step. The samples were analysed by GC-MS/MS, and quantified by matrix-matched calibration. The validation study was carried out on two representative herbs, Chuanxiong Rhizoma and Angelica Sinensis Radix. In two matrices, the linearity of the calibration was good between 5 and 250 ng/mL concentration ranges, and the limits of quantification (LOQs) less than 0.01 mg/kg for most pesticides. At the LOQs and ten times the LOQs, the mean recoveries of almost all pesticides were within 70–120%, with relative standard deviations (RSDs) lower than 10%. The method was applied on twenty real samples. Seven batches of Chuanxiong and five batches of Danggui were found to contain the residues. The combination of modified QuEChERS and GC-MS/MS offers low cost of analysis as well as excellent accuracy and sensitivity. This method could be especially useful for trace analysis of pesticide residues in complex matrices.
Article
A review of literature published in 2014 focusing on analytical methods for pesticides in the water environment is presented here. The review includes publications on extraction methods and on analytical methods such as biochemical assays and immunoassays, electrochemical methods, chromatographic or mass spectrometric techniques, spectrophotometric techniques, fluorescence, and chemiluminescence techniques.
Article
In this study, an ultra-high performance liquid chromatography (UHPLC) coupled to a high resolution Orbitrap mass spectrometry (Orbitrap-HRMS) was demonstrated as a promising technique in high-throughput method development for the routine analysis and contamination control of mycotoxins and pesticide residues in spices. The method was applied for the analysis of fifty ground paprika samples containing blends of sweet and hot paprika harvested in Brazil and China. The efficiency and detection sensitivity of the used UHPLC-Orbitrap-HRMS technique were compared to the results obtained using a triple quadrupole tandem mass spectrometric detector (UHPLC-QqQ-MS/MS). The values of recovery (75–120%) and repeatability (8–15%) for both methods, calculated as the average (n = 5) from the results of spiked (10–500 μg kg−1), paprika samples, were in good conformity to the relevant EU guidelines. The high resolution of the used Orbitrap-HRMS technique provided a better sensitivity for quantitative determination of several pesticide contaminants in paprika, compared to the results obtained by the QqQ-MS/MS method and were comparable in case of mycotoxins. The results of analysis demonstrated the ubiquitous presence of three mycotoxins (fumonisin B1, ochratoxin A, and sterigmatocystin) and twelve pesticide residues in paprika. The concentrations of determined contaminants were below the MRLs set by the Regulations of the European Union with exception of iprovalicarb, which violated the EU MRL in two samples of hot paprika. In addition, a notable difference in the concentration of fumonisin B1 was determined depending on the harvest period (2009–2013), reaching the maximum concentrations of 33 μg kg−1 in sweet paprika and 140 μg kg−1 in hot paprika. There was no significant correlation found between the determined mycotoxin contamination levels and the pesticide residues, with the sole exception of decreased fumonisin B1 content in samples with an elevated concentration of metalaxyl fungicide.
Article
Abstract With the increasing popularity and use of medicinal herbs, their global demand has gained momentum. Developing countries, including China, India and South East Asian (SEA) countries, are the centres of origin and major global suppliers for most of these traditionally used medicinal herbs. One of the factors affecting the quality of these herbs is the contamination of heavy metals, mycotoxins, pesticide residues, polycyclic aromatic hydrocarbons (PAHs) and fumigants. These contaminants can accumulate during the cultivation, storage and processing of herbs and may have adverse effects on consumer health. There have been various reports regarding the presence of these contaminants in medicinal herbs. This review discusses the important contaminants of medicinal herbs, the frequency and magnitude of their occurrences, the potential causes of contamination and their regulatory limits in medicinal herbs. The major challenge in the international trade of medicinal herbs is the lack of common guidelines, regulatory measures and monitoring body to strictly enforce their regulation.
Article
It is widely recognized that the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method is relevant in pesticide residue analysis. Many official laboratories around the globe are routinely using it due to the advantages encapsulated in its name. However, the frontiers of the application of QuEChERS are not yet established. The method is effective for the analysis of other groups of compounds, including pharmaceuticals, mycotoxins, and polycyclic aromatic hydrocarbons, in a wide variety of complex matrices. This review article provides a general overview of the most relevant modifications of the QuEChERS method that have been widely accepted and applied (including both extraction and clean-up) and a general view of the different groups of compounds to which it has been fruitfully applied. We do not include those approaches where only half the method has been used.
Article
Pelargonium graveolens is a valuable source of biologically active compounds and a promising botanical pesticide. In this study, supercritical fluid extraction (SFE) of Pelargonium leaves was optimized to improve the extraction yields, selectivity and pesticidal activity under different operational conditions (pressure 9-30 MPa, temperature 40 and 50 °C). The composition and pesticidal activity of the CO2 extracts were compared with the isolates obtained by maceration and hydrodistillation. GC-MS and GC-FID were used to determine the chemical composition of the isolates. The insecticidal activity (acute and chronic toxicity, antifeedancy) of the isolates was measured on larvae of Spodoptera litoralis. The antifungal activity was evaluated as the inhibition effect on the growth of model pathogenic and toxinogenic fungi (Fusarium oxysporum, Penicillium expansum, Aspergillus fumigatus). The highest yield of CO2 extract was 44.5 mg gplant−1 at 30 MPa, 40 °C and the maximum concentration of the volatiles in extract was 56% w/w at 9 MPa, 50 °C. The insecticidal activity of isolates differed according to the type of test: CO2 extracts obtained at 9 MPa, 50 °C and at 12 MPa, 40 °C exhibited the highest chronic toxicity (LD50 = 6 μg) and antifeedancy (ED50 = 95 μg cm−2), respectively. The essential oil obtained by hydrodistillation, with the yield of 8.5 mg gplant−1 showed the strongest acute toxicity (LD50 = 28 μg). The antifungal activity of isolates increased as the volatile concentration in isolates increased. Results suggest that CO2 extracts of P. graveolens can be suitable substitutes to the essential oil in the use as botanical pesticides.
Article
This study provides, for the first time, data regarding levels of toxic metals (Hg, Cd, and Pb) and organochlorine compounds (PCBs and DDTs) in various aromatic herbs as rosemary (Rosmarinus officinalis), sage (Salvia officinalis), laurel (Laurus nobilis), oregano (Origanum vulgare), and spearmint (Mentha viridis) collected in some towns of the Southern Italy with different anthropogenic and population pressure. Metal and organochlorine compound concentrations were determined using atomic absorption spectrophotometer and gas-chromatography mass spectrometer (GC/MS), respectively. Pb emerged as the most abundant element, followed by Cd and Hg, while between organochlorine compounds, PCB concentrations were higher than those of DDTs. The pollutant concentrations were found to vary depending on the different herbs. The highest Pb levels were observed in rosemary (1.66 μg g(-1) dry weight) and sage (1.41 μg g(-1) dry weight), this latter showing also the highest Cd concentrations (0.75 μg g(-1) dry weight). For PCBs, the major concentrations were found in rosemary (2.75 ng g(-1) dry weight) and oregano (2.39 ng g(-1) dry weight). The principal component analysis applied in order to evaluate possible similarities and/or differences in the contamination levels among sampling sites indicated differences area-specific contamination.
Article
This article highlights some aspects of pesticides contamination in foods and the Government of Nepal's experience in setting MRLs of pesticide on Food. Use of pesticides in agriculture crop has a great concern to all. According to the provision conferred by Food Law, Government of Nepal fixes MRLs of pesticide on food products. Potential products liable for pesticide use gets priority in standard setting. The problem of pesticides begins at the farm level and continues at different stage of handling and storage. Therefore, effective coordination between stakeholders working with different stages of food handling must collaborate to solve this problem. In this connection, some major issues and recommendations in managing proper use of pesticides are highlighted.